Kristall- und Molekülstruktur von Tetra-n-butylammonium-N-methyl-N-thioformyldithiocarbamat

Crystal and Molecular Structure of Tetra-n-butylammonium N-Methyl-N-Thioformyl Dithiocarbamate [N(n-C₄H₉)₄][S₂C? N(CH₃)? CS? H] crystallizes in the triclinic space group P1 (Z = 2) with cell dimensions (?45°C) a = 9.185(2) Å, b = 10.263(3) Å, c = 13.301(3) Å, α = 101.73(2)°, ß = 99.59(2)°, γ 100.57(2)°. The crystal structure was solved by means of direct methods and refined to a conventional reliability index R = 0.066 (R_ω = 0.070). 5945 independent intensities being measured.     

Die Kristall- und Molekülstruktur des Hexaphenyldiplumbans

Crystal and Molecular Structure of Hexaphenyldiplumbane The crystal and molecular structure of (C₆H₅)₆Pb₂ (space group and lattice parameters see above) has been newly determined from 4541 independent reflexes by the heavy atom method; the positions of all atoms, except the H atoms have been refined to give R = 0.053. The unit cell contains two crystallographically independent molecules. (Mean values of bond lengths and angles see above).     

Über Chalkogenolate. 118. Kristall- und Molekülstruktur von Oxovanadin(V)-ethylxanthat

On Chalcogenolates. 118. Crystal and Molecular Structure of Oxovanadium(V) Ethylxanthate VO[S₂C? OC₂H₅]₃ crystallizes with Z = 8 in the monoclinic space group P2₁/n with cell dimensions a = 15.065(7) Å, b = 18.540(48) Å, c = 12.824(7) Å, = 99.31(7)°. The crystal and molecular structure has been determined from single crystal X-ray data at 20°C and refined to a conventional R of 0.045.     

Über Chalkogenolate. 98 [1]. Kristall- und Molekülstruktur von Wolfram(IV)-äthylthioxanthat

On Chalcogenolates. 98. Crystal and Molecular Structure of Tungsten(IV) Ethylthioxanthate W[S₂C? SC₂H₅]₄ crystallizes with Z = 2 in the tetragonal space group P4₂/n with cell dimensions a = 11.108(5) Å and c = 9.489(5) Å. The crystal and molecular structure has been determined from single crystal X-ray data at ?160°C and refined to a conventional R of 0.058. The structure consists of isolated molecules. The tungsten atom is bonded to eight sulfur atoms from four chelating thioxanthate ligands. The coordination geometry approximates very closely to triangularly dodecahedral.     

Die Kristall- und Molekülstruktur des dimeren Dimethylaminodimethylindiums

Crystal and Molecular Structure of Dimeric Dimethylaminodimethylindium Dimeric dimethylamino-dimethylindium was prepared by splitting off methane from the adduct Me₃In? NHMe₂ and characterized by its vibrational spectra. The structure – determined by X-ray analysis – has shown to have the monoclinic space group P2₁/c with a = 7.601, b = 7.336, c = 14.927 Å and β = 119.9°. Patterson, Fourier and Difference synthesis were used for determing the structure, which was refined by least square analysis to an R value of 0.068.     

Das Verhalten von Organosulfonylchloriden gegenüber reinen und substituierten Metallcarbenylen

Mono- and binuclear carbonyls of 5^th, 6^th and 8^th group transition metals react with organosulfonyl chlorides, RSO₂Cl, to form organosulfinato metal chlorides with, in the case of electronegative R (R = CF₃), metal(II) and, in the case of electropositive (R = p?CH₃C₆H₄), metal(II) or (III). Bis(organosulfinato) complexes are obtainable from metal(II) chlorides and sodium organosulfinates. In all these new sulfinato compounds the ligand is bound to the metal through both its oxygen atoms; this is deduced from the IR spectra.     

Kristall- und Molekülstruktur von Bis(pyridin)bis(trifluoromethyl)zink

Crystal and Molecular Structure of Bis(pyridine)bis(trifluoromethyl)zinc Bis(pyridin)bis(trifluoromethyl)zinc 1 has been isolated and characterized by means of single-crystal X-ray diffraction techniques. The title compound represents the first structure determination of a fully fluorinated alkylzinc compound (monoclinic, space group P2₁/c, Z = 4, a = 8.856(3), b = 18.158(3), c = 8.979(3) Å, β = 98.14(2)°, R = 0.054, R_w = 0.035). The zinc atom is in a distorted tetrahedral environment. The molecular structure of [ClZn(CCl₂CF₃) η₂O]₂ 2 was solved, but is not included in a structural comparison due to crystallographic disorder.     

Schwefel(IV)-Verbindungen als Liganden. II. Die Kristall- und Molekülstruktur von Pentacarbonyl-(schwefeldioxid)chrom

Sulfur(IV) Compounds as Ligands. II. The Crystal and Molecular Structure of Pentacarbonyl--(sulfur dioxide)chromium The structure of pentacarbonyl(sulfurdioxide)chromium ( 1 ) has been determined from single crystal X-ray data. The compound crystallizes with eight formula units in the rhombic unit cell (space group Pbn2₁) of the dimensions a = 657.8(2) pm, b = 1245.2(4) pm, c = 2177.4(5) pm (at 180 K). The sulfur dioxide is η¹-coplanar coordinated, the Cr? S distance is 219 pm, the shortest bond reported so far between chromium(0) and sulfur. The Cr? C(ax) bond (189 pm) was found only marginally shorter than the Cr? C(eq) bonds (190 pm) providing proof of the high π-acceptor capacity of SO₂.     

Kristall- und Molekülstruktur von Bis[N-(diethylaminothiocarbonyl)-benzamidin]silber(l)-nitrat

Crystal and Molecular Structure of Bis[N-(diethylaminothiocarbonyl)-benzamidine]-silver(I) Nitrate The crystal structure of bis[N-(diethylaminothiocarbonyl)-benzamidine]silver(I) nitrate has been determined by X-ray structure analysis on a single crystal. The compound is monoclinic, space group P2₁/n with a = 12.541, b = 43.470, c = 11.096 Å, β = 106.27° and 8 formula units per unit cell. The structure was solved by application of direct methods to difference structure factors (DIRDIF) and refined for 5242 observed reflections to a final R value of R = 0.070. There are two symmetrically independent molecules of the title compound in the asymmetric unit. The central Ag ion is coordinated by the S atoms of two ligands. The nitrate ions do not coordinate. The coordination geometry is slightly bent.     

Bis[bis(trimethylsilyl)amino]sulfan 2. Kristall- und Molekülstruktur

Bis[bis(trimethylsilyl)amino]sulfane. 2. Crystal and Molecular Structure The title compound [(CH₃)₃Si]₂N? S? N[Si(CH₃)₃]₂ crystallizes with Z = 4 in the monoclinic space group A2/a (Nr. 15) with cell dimensions a = 22.436(4) Å, b = 6.434(5) Å, c = 17.089(6) Å, β = 117.66(2)º. For 5091 independent reflections, measured at ?80°C, the structure could be refined to R = 0.079 and R_w = 0.120. The molecules are linked together by van der Waals interactions and form layers in the bc plane, in agreement with the observed cleavage along (100).     

Die Kristall- und Molekülstruktur von Dicäsium- μ-Oxodekafluorodiarsenat

Crystal and Molecular Structure of Dicaesium-μ-Oxodecafluorodiarsenate, Cs₂(As₂F₁₀O) The crystal structure of Cs₂(As₂F₁₀O) has been determined from three-dimensional data. The compound crystallizes in the monoclinic space group P2₁/m, the lattice constants being a = 9.175(4), b = 10.690(5), c = 5.619(3)(Å); β = 105,50(5)°. The anion (As₂F₁₀O)^2– with the point symmetry C_s contains a As? O? As-bridge, whose partial π-bonding is to be discussed. The bond lengths and angles are: As? O: 1.77(2) and 1.68(2) Å, resp., As? O? As: 139(1)°; As…As: 3.225(4) Å, the numbers in parantheses being the standard deviation of the last figure.     

Kristall- und Molekülstruktur von Bis[N-(diethylaminothiocarbonyl)-N′-phenylbenzamidinato]nickel(II)

Crystal and Molecular Structure of Bis[N-(diethylaminothiocarbonyl)-N′-phenyl-benz-amidinato]nickel(II) The structure of bis[N-(diethylaminothiocarbonyl)-N′-phenyl-benzamidinato]-nickel(II) has been determined by X-ray structure analysis. The compound crystallizes in orthorhombic space group P2₁2₁2₁ with a = 16.36, b = 16.94, c = 12.96 Å and Z = 4. The solution of the structure was performed by heavy atom technique and gave a final R value of R = 0.055 for 1764 observed reflections. The coordination polyhedron has a tetrahedrally distorted shape. The ligator atoms are arranged in cis position. The chelate rings deviate clearly from planarity. Against the chelate rings the phenyl rings are appreciably twisted. The title compound is compared regarding its structure with the analogous copper chelate.     

Synthese sowie Kristall- und Molekülstruktur von Tetrafluoro[2-(pyrrolidinio)ethyl]silicat

Synthesis and Crystal and Molecular Structure of Tetrafluoro[2-(pyrrolidinio)ethyl]silicate The zwitterionic tetrafluoro[2-(pyrrolidinio)ethyl]silicate ( 4 ) was synthesized by reaction of trimethoxy(2-pyrrolidinoethyl)silane ( 5 ) with hydrogen fluoride in ethanol/hydrofluoric acid at 0°C. The crystal and molecular structure of 4 was studied at ?100°C by single-crystal X-ray diffraction. In addition, 4 was characterized by solution-state NMR studies (CD₃CN: ¹H, ¹³C).